GB/T 22729-2008 PDF English
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Oligopeptides powder of marine fish
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GB/T 22729-2008: PDF in English (GBT 22729-2008) GB/T 22729-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
X 80
Oligopeptides powder of marine fish
海洋鱼低聚肽粉
ISSUED ON: DECEMBER 31, 2008
IMPLEMENTED ON: AUGUST 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 5
4 Product classifications ... 5
5 Technical requirements ... 6
6 Test method ... 7
7 Inspection rules ... 11
8 Labeling, packaging, transportation, storage ... 13
Appendix A (Normative) Proportion of protein hydrolysates with relative
molecular mass less than 1000 u (High performance gel filtration
chromatography) ... 14
Oligopeptides powder of marine fish
1 Scope
This standard specifies the product classification, technical requirements, test
methods, inspection rules, labeling, packaging, transportation, storage of
oligopeptide powder of marine fish.
This standard applies to the production, inspection, sales of oligopeptide
powder products of marine fish.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB 2733 Hygienic standard for fresh and frozen marine products of animal
origin
GB/T 4789.2 Microbiological examination of food hygiene - Aerobic plate
count
GB/T 4789.3 Microbiological examination of food hygiene - Detection of
Coliform bacteria
GB/T 4789.4 Microbiological examination of food hygiene - Examination of
Salmonella
GB/T 4789.5 Microbiological examination of food hygiene - Examination of
Shigella
GB/T 4789.10 Microbiological examination of food hygiene - Examination of
staphylococcus aureus
GB/T 4789.15 Microbiological examination of food hygiene - Examination of
molds and yeasts
GB/T 5009.3 Determination of moisture in food
results are not converted into protein coefficients. They are expressed in terms
of total nitrogen mass fraction.
6.3 Oligopeptides
6.3.1 Method summary
Low-molecular-weight protein hydrolysates (including oligopeptides and free
amino acids) are soluble in trichloroacetic acid solution. The high-molecular-
weight proteins are easy to precipitate in trichloroacetic acid solution. After the
sample is dissolved in the trichloroacetic acid solution, it is centrifuged, to
separate the precipitated protein. Collect the centrifuged supernatant.
According to the method specified in GB/T 5009.5, determine the acid-soluble
protein hydrolysate content of the centrifuged supernatant. The acid-soluble
protein hydrolysate content minus the free amino acid content, to obtain the
content of oligopeptides.
6.3.2 Analytical procedures
6.3.2.1 Determination of acid-soluble protein hydrolysate content
Weigh 2 g (accurate to 0.001 g) of sample. Add 10 mL of 15% trichloroacetic
acid solution. Mix well. Let it stand for 10 min. After centrifuging the sample
solution for 10 min at 4000 r/min, take all the centrifuged supernatant.
Determine the protein hydrolysate content of the supernatant, according to the
method specified in GB/T 5009.5. Calculate the acid-soluble protein
hydrolysate content in the sample. The protein conversion factor is 6.25. The
test results are converted to a dry basis, based on the loss on drying of the
sample.
6.3.2.2 Determination of free amino acid content
6.3.2.2.1 Determination method by amino acid automatic analyzer
Weigh 0.02 g ~ 0.03 g of sample, accurate to 0.0001 g. Use 3.5% sulfosalicylic
acid solution, to dissolve it evenly. Transfer the sample solution into a 50 mL
volumetric flask. Make the volume constant. Centrifuge the sample solution for
5 min, in a centrifuge, at a speed of 4000 r/min. Take the centrifuged
supernatant. Then use a 0.45 μm microporous filter membrane, to filter the
centrifuged supernatant. Transfer the filtrate into a 50 mL volumetric flask. Make
its volume reach to the mark; shake it uniformly to prepare for use. Then
determine its free amino acid content, by an automatic amino acid analyzer, in
accordance with the method specified in GB/T 5009.124.
6.3.2.2.2 Determination by high performance liquid chromatograph
6.3.2.2.2.1 Method summary
After precipitating the protein with trichloroacetic acid, use o-phthalaldehyde
(OPA) and fluorene methyl chloroformate (FMOC-Cl) as the derivatization
reagents, for primary and secondary amino acids, respectively. Use the pre-
column automatic derivatization reversed-phase high-efficiency liquid
chromatography, to determine the total free amino acids in oligopeptide powder
of marine fish.
6.3.2.2.2.2 Instruments
a) High performance liquid chromatograph: It is equipped with quaternary
gradient pump, UV detector, autosampler, ChemStation software, online
degasser.
b) Analytical balance: Sensitivity 0. 0001 g.
c) pH meter.
6.3.2.2.2.3 Reagents
Triethylamine, tetrahydrofuran, acetic acid, boric acid are all analytically pure;
methanol, acetonitrile, amino acid standards, o-phthalaldehyde (OPA), fluorene
methyl chloroformate (FMOC-Cl) are all chromatographically pure; ultrapure
water.
6.3.2.2.2.4 Determination
Weigh the 0.5 g of sample, accurate to 0.0001 g. Add 10 mL of 5%
trichloroacetic acid to a 25 mL volumetric flask, to precipitate for 2 hours. Make
its volume reach to the mark. Shake it uniformly. Filter it. Centrifuge at 10000
r/min for 15 min. Take the supernatant. Load it in the machine. Use an external
standard method for determination.
Chromatographic conditions: Analytical column: Hypersil AA-ODS, 5 μm, 200
mm × 2.1 mm (inner diameter). Mobile phase: Solution A: The 20 mmol/L
sodium acetate buffer, which contains 0.018% triethylamine (TEA); use dilute
acetic acid to adjust to pH7.2; add 0.3% tetrahydrofuran (THF). Solution B: The
100 mmol/L sodium acetate buffer solution of 20%; use dilute acetic acid to
adjust to pH7.2; add 40% acetonitrile and 40% methanol. Gradient elution
program: The solution A is 100% at 0 min; the solution B is from 0% to 60%
within 17 min. The solution B is 100% at 18 min, which is kept to 24 min. At 25
min, the solution B returns to 0%. Flow rate: 0.45 mL/min before 18.1 min; it
rises to 0.8 mL/min at 18.5 min, which is kept to 23.9 min; at 24 min, it drops
back to 0.45 mL/min. UV detection: Use 338 nm for the determination of primary
amino acids AND 262 nm for the determination of secondary amino acids (after
15 min). Fluorescence detection: Determine the excitation wavelength of the
primary amino acid at 340 nm AND the emission wavelength at 450 nm; after
14.5 min, the wavelength is switched to 266 nm (excitation) and 305 nm
Measure in accordance with the method specified in GB/T 5009.15.
6.12 Methyl-mercury
Measure in accordance with the method specified in GB/T 5009.17.
6.13 Total number of colonies
Measure in accordance with the method specified in GB/T 4789.2.
6.14 Coliform flora
Measure in accordance with the method specified in GB/T 4789.3.
6.15 Molds and yeasts
Measure in accordance with the method specified in GB/T 4789.15.
6.16 Pathogenic bacteria
Salmonella, Shigella and Staphylococcus aureus are tested according to the
methods, which are specified in GB/T 4789.4, GB/T 4789.5, GB/T 4789.10,
respectively.
7 Inspection rules
7.1 Inspection classification
7.1.1 Exit-factory inspection
The items of the exit-factory inspection include sensory characteristics, total
nitrogen, oligopeptides, proportion of protein hydrolysates with a relative
molecular weight of less than 1000 u, loss on drying, ash content (except
collagen oligopeptide powder of marine fish bone), the total number of colonies,
coliform flora.
7.1.2 Type inspection
Type inspection items include all the items, which are specified in 5.2, 5.3, 5.4,
5.5.
For the products, which are produced throughout the year, they shall be type-
inspected once a year. However, they shall also be type-inspected in any of the
following situations:
- When the new product is put into production;
- When there are major changes in raw materials and processes;
7.3.2.2 In the type inspection items, if the microbial indicators do not meet this
standard OR if malignant impurities (such as glass, metal, insects, etc.) are
found, they shall not be re-inspected BUT judged as unqualified products.
7.3.2.3 In the type inspection items, except for the indicator as mentioned in
7.3.2, if other indicators do not meet this standard, it may double sampling from
the same batch of products, to re-inspect the unqualified items. If the result of
the re-inspection still does not meet the requirements of this standard, it will be
judged as unqualified product.
8 Labeling, packaging, transportation, storage
8.1 Label
8.1.1 The product label shall indicate the product name, net content, name and
address of the manufacturer and distributor, production date, production batch
number, shelf life, product standard number, etc.
8.1.2 The product name shall meet the requirements in Chapter 4.
8.2 Packaging
The packaging container shall meet the hygienic standards of food containers
and packaging materials.
8.3 Transportation
The tools and vehicles, which are used to transport products, shall be clean,
hygienic, dry and free of pollutants. During the transportation of the product, it
shall be covered, protected from rain and sun exposure. It cannot be mix-
transported with toxic, harmful, or odorous items.
8.4 Storage
8.4.1 Products shall not be stacked in the open. The finished product
warehouse shall be clean, dry, ventilated, free of rodents and insects.
8.4.2 The product shall be stacked with backing plates. It shall be more than 10
cm above the ground and 20 cm away from the wall.
8.4.3 Products shall not be stored in the same warehouse, with toxic, harmful,
odorous, perishable, or damp items.
detector AND chromatographic workstation or integrator, with GPC data
processing software.
A.3.2 Mobile phase vacuum filtration and degassing device.
A.3.3 Ultrasonic oscillator.
A.3.4 Analytical balance: Sensitivity 0. 0001 g.
A.4 Chromatographic conditions and system adaptability experiment
Chromatographic column: TSKgel G2000 SWXL 300 mm × 7.8 mm or other gel
columns of similar performance, suitable for the determination of proteins and
peptides.
Mobile phase: Acetonitrile: water: trifluoroacetic acid is 45:55:0.1 (volume ratio).
Detection wavelength: UV220 nm.
Flow rate: 0.5 mL/min.
Column temperature: 30 °C.
Injection volume: 10 μL.
In order to make the chromatographic system meet the detection requirements,
it is stipulated that, under the above chromatographic conditions, the column
efficiency of the gel chromatography column, that is, the number of theoretical
plates (N), is calculated based on the peak of the tripeptide standard (Gly-Gly-
Gly), which is not less than 5000; the distribution coefficient (Kd) of
oligopeptides shall be within 0 ~ 1.
A.5 Preparation of relative molecular mass calibration curve
Respectively, use the mobile phase to prepare 0.1% (mass concentration)
above-mentioned peptide standard solutions of different relative molecular
mass. After filtering with polytetrafluoroethylene or nylon filter membrane, which
has a pore diameter of 0.2 μm ~ 0.5 μm, make sample injection, respectively,
to obtain the chromatograms of the series of standard products. Use the
logarithm of the relative molecular mass (lgMr) to plot the retention time, OR
make a linear regression, to obtain the relative molecular mass calibration curve
and its equation.
A.6 Sample preparation
Weigh 20.0 mg of sample, in a 10 mL volumetric flask. Use mobile phase to
dilute the volume to the mark. Oscillate ultrasonically for 10 min, to dissolve and
mix the sample thoroughly. After filtering by polytetrafluoroethylene or nylon
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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